Method of impregnating protective clothing



United States Patent METHOD OF INIPREGNATING PROTECTIVE CLOTHING SourenZ. Avedikian, Larclimont, N.Y., assignor to the United States of Americaas represented by the Secretary of War in trust N0 Drawing. ApplicationFebruary 12, 1942 Serial No. 430,690

, 16 Claims. (Cl. 117-161) (Granted under Title 35, U8. Code (1952),see. 266) The invention described herein may be manufactured and used byor for the Government for governmental purposes, without the payment tome of any royalty thereon.

This invention relates generally to certain improvements in protectiveclothing adapted to give protection against mustard gas and likechemical warfare vesicants, and to certain improvements in methods ofmaking such protective clothing.

More particularly, this invention relates to the type of protectiveclothing known to those skilled in the art as permeable protectiveclothing. This type of protective clothing is permeable to air andmoisture and is adapted to have substantially the same wearingcharacteristics as ordinary clothing. Such permeable protective clothingis distinguished from the other recogniied type of protective clothingwhich is known to those skilled in the art as impermeable protectiveclothing. This latter type of protective clothing is impervious to allgases and cannot be worn for long periods of time because it does notpermit body perspiration. Impermeable protective clothing is used on asmall scale in decontamination work where high vesicant concentrationsare encountered.

It has been found that mustard gas and like vesicants can be renderedsubstantially harmless by halogenation or chlorination so as to convertthe vesicant agents into ,non-irritant products. A number of organiccompounds containing available halogen atoms are known which, in variousdegrees, are capable of chlorinating mustard gas. The chloraminescontaining available chlorine are, as a class, suitable for thispurpose. When these compounds are used as the active agents inprotective clothing they are usually referred to as impregnites. Thefollowing table is a list of a number of compounds which have been usedor suggested as impregnating agents for protective clothing:

Of the foregoing compounds, bis 2,4,6-trichlorphenyl chlorurea has beenfound to be particularly well suited as an impregnating agent.

However, considerable difiiculty has been encountered in incorporatingthe impregnating agents into, or binding them to, fabric or cloth so asto provide satisfactory protective clothing which closely resemblesordinary untreated clothing. Various types of binders for theimpregnites have been suggested, none of which has proven entirelysatisfactory. The principal objections to protective clothing providedheretofore have been that: (1) it was tacky and sticky so as to beuncomfortable to put on and wear; (2) considerable shrinkage occurredwhen a garment was treated so as to convert it into protective clothing;and (3) the protective clothing deteriorated appreciably during storageand repeated washing. In addition to the foregoing objectionableproperties of protective clothing, heretofore it was necessary to carryout the impregnation treatment at elevated temperatures.

Accordingly, a primary object of this invention, generally stated, isthe provision of protective clothing of the type described wherein: (1)tackiness or stickiness is substantially eliminated; (2) which is freefrom shrinkage; and (3) which retains its initial high protectiveproperty in a high degree without deterioration over long periods oftime even when subjected to repeated washings. Another important objectof this invention is the provision of a method of making protectiveclothing without shrinkage of the fabric or garment during treatment.

Still another important object of this invention is the provision of amethod of impregnating fabric or clothing at ordinary room temperaturesso as to render the same impermeable to mustard gas and the like.

Other objects of my invention will, in part, be obvious,-

and in part appear hereinafter.

In brief, the invention involves the use of a binder comprising a vinyltype polymerization product, or a socalled Vinylite, and a suitableplasticizer therefor, to bind and incorporate an impregnating agent oranti-vesicant agent into clothing or fabric. Specifically, it has beenfound that a binder comprising the polyvinyl acetate polymerizationproduct known commercially as Vinylite A (Carbide and Carbon Chem.Corp.) and dibutyl phthalate as a plasticizer therefor, is particularlywell adapted to bind and incorporate the impregnating agent, bis2,4,6-trichlorphenyl chlorurea, into fabric or clothing so as to providesuperior protective clothing and garments, highly resistant to mustard.gas and like vesicants. Protective clothing made with this combinationName Formula Percent A cti ve Chlorine Phthal-chloramide CJMCOMNGhlorortho henzoic sulfinide CrlliCO(SO )NOl Quinone dichlorimid Cal-MNl)? Chlorsuccinimide Dihenzoyl ethylene dichlo Benzoy] chlorcarbamide CHSCONHC Dihenzovlyrlichlorcarba (CuH5CONCl)zCO. Iodobenzene dichloride.CGTI5IGI2 Bis(dichlorphenylchlor)urea CH3CON(Cl)C5H2Cl3 C HsCO1(Cl)C5llgcla of binder and impregnating agent is particularlydistinguished by the absence of shrinkage on impregnation, its freedomfrom stickiness and tackiness, and its high resistance to deterioration.

For a more complete understanding of the nature and scope of thisinvention reference may be had to the following detailed illustrativedescription thereof.

Any ordinary type of fabric, such as cotton, wool, or mixtures thereof,may be treated according to this invention either before or after it hasbeen made into garments. The impregnating agent and binder may beapplied to the fabric or clothing in the form of a solution thereof in avolatile solvent. A solution of the following composition has given goodresults in practice:

Vinylite A (Carbide and Carbon Chem. Corp.) 1% by weight.

Plasticizer 1% by weight (dibutyl phthalate).

Volatile solvent 91% by weight (acetylene tetrachloride).

Protective agent 7% by weight (bis 2-4- 6 trichlorphenyl chlorurea).

It will be understood that the foregoing composition may be variedwithin limits and that the constituents may be replaced by variousequivalent materials. For example, the acetylene tetrachloride may bereplaced by chlorobenzene or any other suitable volatile solvent inwhich the ingredients are sufficiently soluble and which is inertthereto. Likewise the bis 2-4-6 trichlorphenyl chlorurea may be entirelyor partially replaced by bis dichlorphenyl chlorurea. The Vinylite maybe used in amounts up to by weight, or even greater, and the protectiveagent may be used in amounts up to the limit of its solubility in thesolvent, and even in amounts exceeding its solubility if measures aretaken to thoroughly agitate the mixture so as to maintain an intimatemixture and dispersion of the solid phase throughout the solution duringimpregnation.

One satisfactory method of treating fabric or garments with the above orequivalent solutions is to immerse the fabric or garments in a bath ofthe solution at room temperature so as to thoroughly wet the same. Thenthe fabric or garments may be removed from the bath and excess liquidremoved therefrom either by wringing or centrifuging the same.Thereafter, the fabric or garments may be allowed to dry so as tocomplete the removal of the volatile solvent and leave the impregnatingagent and binder firmly incorporated in the fibers.

Care should be taken to remove as much of the excess liquid as can beconveniently done by wringing or centrifuging so as to keep the increasein weight of the fabric or garment due to impregnation to a minimum andat the same time prevent the unnecessary closing oif of the intersticesand openings between the fibers.

It will be understood that certain other metho'ds and techniques may beemployed to treat fabric and clothing with the impregnating solutions.

Cloth impregnated with a solution having the composition outlbined aboveand according to the foregoing method will have the followingapproximate composition with regard to the materials added:

Total materials added, (i.e., increase in 25 to 28% of the weight ofuntreated cloth.) original weight.

Percentage of binder and protective agent in treated cloth 2022%.Percentage of binder 3-5 Percentage of protective agent 17+%.

The unexpected resistance to deterioration of protective clothing madeaccording to this invention is thought to be due in large measure to thefact that the Vinylite type of binder not only serves to bind theprotective 4 agent into the fabric, but that it also serves as a protec:tive agent for the fibers of the clothing or fabric.

Since certain changes may be made in the foregoing compositions,percentages, and techniques of application without departing from thescope of the invention, it is intended that all matter described abovebe interpreted as illustrative and not in a limiting sense.

I claim:

1. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants susceptible of being rendered non-vesicant bychlorination, which comprises, impregnating the fabric or clothing withhis 2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising avinyl ester polymerization product.

2. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants susceptible of being rendered non-vesicant bychlorination, which comprises, impregnating the fabric or clothing withhis 2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising avinyl ester polymerization product and a plasticizer therefor.

33. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants, susceptible of being rendered non-vesicant bychlorination, which comprises, impregnating the fabric or clothing withhis 2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising avinyl ester polymerization product and dibutyl phthalate.

4. The method providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants susceptible of being rendered non-vesicant bychlorination, which comprises, impregnating the fabric or clothing atroom temperature with bis 2,4,6-trichlorphenyl chlorurea incorporated ina binder comprising a vinyl ester polymerization product and aplasticizer therefor.

5. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants, which comprises, wetting fabric or clothing with asolution of bis 2,4,6-trichlorphenyl chlorurea and a binder comprising avinyl ester polymerization product and dibutyl phthalate, removingexcess of said solution from the wetted fabric or clothing, and dryingthe treated fabric or clothing.

6. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants, which comprises, wetting fabric or clothing at roomtemperature with an intimate mixture of his 2,4,6-trichlorphenylchlorurea and a binder comprising polyvinyl acetate and a plasticizertherefor, in acetylene tetrachloride, removing excess of said intimatemixture from the wetted fabric or clothing, and drying the treatedfabric or clothing so as to remove acetylene tetrachloride solventtherefrom.

7. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants, which comprises, wetting fabric or clothing at roomtemperature with a solution comprising by weight about 7% of his2,4,6-trichlorphenyl chlorurea, about 2% by weight of a bindercomprising approximately equal parts of a vinyl ester polymerizationproduct and dibutyl phthalate plasticizer therefor in about 91% byweight of acetylene tetrachloride, removing excess of said solution fromthe wetted fabric or clothing, and drying the treated fabric or clothingso as to remove acetylene tetrachloride solvent therefrom.

8. The method of providing, without substantial shrinkage, non-tacky,air-permeable protective fabric and clothing resistant to mustard gasand like vesicants,

which comprises, wetting fabric or clothing at room temperature with asolution comprising by weight about 7% of bis 2,4,6-trichlorphenylchlorurea, about 2% by weight of a binder comprising approximately equalparts of polyvinyl acetate and dibutyl phthalate plasticizer therefor,in about 91% by weight of acetylene tetrachloride, removing excess ofsaid solution from the wetted fabric or clothing, and drying the treatedfabric or clothing so as to remove acetylene tetrachloride solventtherefrom.

9. Protective clothing impermeable to mustard gas and like vesicantssusceptible of being rendered nonvesicant by chlorination, andcharacterized by being non-tacky, air-permeable, and relativelycomfortable to wear, and made from fabric impregnated with his 2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising a vinylester polymerization product.

10. Protective clothing impermeable to mustard gas and like vesicantssusceptible of being rendered nonvesicant by chlorination, andcharacterized by being nontacky, air-permeable, and relativelycomfortable to wear, and made from fabric impregnated with bis2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising avinyl ester polymerization product and plasticizer therefor.

11. Protective clothing impermeable to mustard gas and like vesicantssusceptible of being rendered nonvesicant by chlorination, andcharacterized by being nontacky, air-permeable, and relativelycomfortable to wear, and made from fabric impregnated with bis2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising avinyl ester polymerization product and dibutyl phthalate.

12. Protective clothing impermeable to mustard gas and like vesicantssusceptible of being rendered nonvesicant by chlorination, andcharacterized by being non-tacky, air-permeable, and relativelycomfortable to wear, and made from fabric impregnated with his 2,4,6-trichlorphenyl chlorurea incorporated in a binder comprising a vinylester polymerization product and dibutyl phthalate, said bis2,4,6-trichlorphenyl chlorurea being present in an amount equal to about15% to 17% of the weight of the fabric, and said binder being present inan amount equal to about 3% to 5% of the weight of the fabric.

13. A fabric impregnating composition for rendering fabric and clothingimpermeable to mustard gas and like vesicants susceptible of beingrendered non-vesicant by chlorination but permeable to air, whichcomprises, an intimate mixture of bis 2,4,6-trichlorphenyl chlorurea anda binder comprising a vinyl ester polymerization product and plasticizertherefor, in a volatile solvent.

14. A fabric impregnating composition for rendering fabric and clothingimpermeable to mustard gas and like vesicants susceptible of beingrendered non-vesicant by chlorination but permeable to air, whichcomprises an intimate mixture of his 2,4,6-trichlorphenyl chlorurea anda binder comprising polyvinyl acetate and a plasticizer therefor, in avolatile solvent.

15. A fabric impregnating composition for rendering fabric and clothingimpermeable to mustard gas and like vesicants susceptible of beingrendered non-vesicant by chlorination but permeable to air, whichcomprises an intimate mixture of his 2,4,6-trichlorphenyl chlorurea anda binder comprising polyvinyl acetate and dibutyl phthalate, inacetylene tetrachloride.

16. A fabric impregnating composition for rendering fabric and clothingimpermeable to mustard gas and like vesicants susceptible of beingrendered non-vesicant by chlorination but permeable to air, whichcomprises a solution of about 7% by weight of his 2,4,6-trichlorphenylchlorurea and about 2% by weight of a binder comprising approximatelyequal parts of polyvinyl acctate and dibutyl phthalate, in about 91% byweight of acetylene tetrachloride.

References Cited in the file of this patent UNITED STATES PATENTS2,173,781 Gibells Sept. 19, 1939 FOREIGN PATENTS 373,947 Great BritainJune 2, 1932 448,164 Great Britain June 3, 1936 486,162 Great BritainMay 31, 1938

1. THE METHOD OF PROVIDING, WITHOUT SUBSTANTIAL CLOTHING, NON-TACKY,AIR-PERMEABLE PROTECTIVE FABRICS AND CLOTHING RESISTANT TO MUSTARD GASAND LIKE VESICANTS SUSCEPTIBLE OF BEING RENDERED NON-VESICANT BYCHLORINATION, WHICH COMPRISES, IMPREGNATING THE FABRIC OR CLOTHING WITHBIS 2,4,6-TRICHLORPHENYL CHLORUREA INCORPORATED IN A BINDER COMPRISING AVINYL ESTER POLYMERIZATION PRODUCT.